Hexahydro-1,4-diazepine → 3-(1-Homopiperazinyl)-6-methoxy-1,2-benzisoxazole

HRID 1939159Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1939159
Cl[C:2]1[C:6]2[CH:7]=[CH:8][C:9]([O:11][CH3:12])=[CH:10][C:5]=2[O:4][N:3]=1.[NH:13]1[CH2:19][CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1>CCOC(C)=O>[N:13]1([C:2]2[C:6]3[CH:7]=[CH:8][C:9]([O:11][CH3:12])=[CH:10][C:5]=3[O:4][N:3]=2)[CH2:19][CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1

Komponenten

4

Edukt 2

HCID 68163Hexahydro-1,4-diazepineHCID 158169243-Chloro-6-methoxy-1,2-benzoxazole

Produkt 1

HCID 218393333-(1-Homopiperazinyl)-6-methoxy-1,2-benzisoxazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

3-Chloro-6-methoxy-1,2-benzisoxazole (5.0 g, 27.2 mml) and homopiperazine (8.2 g, 81.6 mmol) were combined and mechanically stirred under N2 at 140° C. for 45 minutes. The reaction mixture was cooled to room temperature, dissolved with EtOAc (500 ml), and the solution was washed with water, brine, dried over MgSO4, and concentrated in vacuo. Flash column chromatography (silica gel, 20% MeOH/CH2Cl2) provided the product (2.0 g, m.p. 74°-75° C.

Aufarbeitung

  1. temperatureThe reaction mixture was cooled to room temperature
  2. washthe solution was washed with water, brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customFlash column chromatography (silica gel, 20% MeOH/CH2Cl2) provided the product (2.0 g, m.p. 74°-75° C.

Quellen und Nachweise

ORD-Eintrag
ord-ca355c11390341bba2df964c724a2327
Quelldatensatz
uspto-grants-1997_12
Patentnummer
US05696113

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